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81. 发明授权

US5906956A Lithium initiator system 失效
标题翻译：锂引发剂体系
公开(公告)号：US5906956A
公开(公告)日：1999-05-25
申请号：US834787
申请日：1997-04-03
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F4/48 , C08F136/06 , C08F136/08
CPC分类号： C08F136/08 , C08F136/06
摘要： This invention reveals an initiator system which is comprised of (a) a lithium initiator, (b) a sodium alkoxide and (c) a polar modifier; wherein the molar ratio of the sodium alkoxide to the lithium initiator is within the range of about 0.05:1 to about 3:1; and wherein the molar ratio of the polar modifier to the lithium initiator is within the range of about 0.25:1 to about 5:1. The subject invention also discloses a process for preparing 3,4-polyisoprene rubber which comprises polymerizing isoprene monomer with a lithium initiator at a temperature which is within the range of about 30.degree. C. to about 100.degree. C. in the presence of a sodium alkoxide and a polar modifier, wherein the molar ratio of the sodium alkoxide to the lithium initiator is within the range of about 0.05:1 to about 3:1; and wherein the molar ratio of the polar modifier to the lithium initiator is within the range of about 0.25:1 to about 5:1.
摘要翻译：本发明揭示了一种引发剂体系，其包括（a）锂引发剂，（b）醇钠和（c）极性改性剂; 其中所述醇钠与所述锂引发剂的摩尔比在约0.05:1至约3:1的范围内; 并且其中极性改性剂与锂引发剂的摩尔比在约0.25:1至约5:1的范围内。本发明还公开了一种制备3,4-聚异戊二烯橡胶的方法，该方法包括在钠存在下，在约30℃至约100℃的温度范围内用锂引发剂聚合异戊二烯单体醇盐和极性改性剂，其中烷氧基钠与锂引发剂的摩尔比在约0.05:1至约3:1的范围内; 并且其中极性改性剂与锂引发剂的摩尔比在约0.25:1至约5:1的范围内。

82. 发明授权

US07825195B2 Dendrimers of rubbery polymers 失效
标题翻译：橡胶聚合物的树枝状聚合物
公开(公告)号：US07825195B2
公开(公告)日：2010-11-02
申请号：US12611807
申请日：2009-11-03
申请人： Adel Farhan Halasa , Wen-Liang Hsu , Chad Aaron Jasiunas
发明人： Adel Farhan Halasa , Wen-Liang Hsu , Chad Aaron Jasiunas
IPC分类号： C08C19/25 , C08F8/18 , C08F36/04 , C08J3/24 , B60C1/00
CPC分类号： C08C19/44 , B60C1/0016 , C08G83/003 , C08L15/00 , C08L101/005 , Y10T152/10 , Y10T152/10495
摘要： This invention discloses a process for synthesizing a dendrimer of a rubbery polymer comprising: (a) reacting a lithium terminated rubbery polymer with a halogenated silicon containing compound to produce a polymer which is terminated with halogenated silicon moieties, wherein the halogenated silicon contain compound has at least four halogen atoms which are bonded directly to silicon atoms, wherein the ratio of the lithium terminated rubbery polymer to halogen atoms in the halogenated silicon containing compound is within the range of 2:n to (n-1):n, wherein n represents the number of halogen atoms that are bonded directly to silicon atoms in the halogenated silicon containing compound, wherein the halogenated silicon containing compound contains at least three halogen atoms which are bonded directly to a silicon atom; (b) reacting the polymer which is terminated with halogenated silicon moieties with a molar excess of a tertiary alcohol to produce a polymer which is terminated with hydroxy silyl moieties; and (c) allowing the polymer which is terminated with the hydroxy silyl moieties to couple under conditions sufficient to produce a dendrimer containing siloxane linkages. It has also be found that similar dendrimers having improved processability can be make utilizing halogenated tin containing compounds in stead of the halogenated silicon containing compound.
摘要翻译：本发明公开了一种用于合成橡胶状聚合物树枝状聚合物的方法，其包括：（a）使锂封端的橡胶状聚合物与含卤化硅的化合物反应以制备用卤化硅部分封端的聚合物，其中卤化硅含有化合物在至少四个与硅原子直接键合的卤素原子，其中锂封端的橡胶状聚合物与含卤化硅化合物中的卤素原子的比例在2：n至（n-1）：n的范围内，其中n表示与卤代硅化合物中的硅原子直接键合的卤素原子数，其中含卤化硅的化合物含有至少三个与硅原子直接键合的卤素原子; （b）将用卤代硅部分封端的聚合物与摩尔过量的叔醇反应，以产生用羟基甲硅烷基部分封端的聚合物; 和（c）使在羟基甲硅烷基部分封端的聚合物在足以产生含有硅氧烷键的树枝状聚合物的条件下偶联。还可以发现，具有改进加工性能的类似树枝状大分子可以利用含卤化锡的化合物代替含卤化硅的化合物。

83. 发明授权

US07671237B2 Synthesis of soluble functionalized lithium initiators 失效
标题翻译：可溶性官能化锂引发剂的合成
公开(公告)号：US07671237B2
公开(公告)日：2010-03-02
申请号：US11479717
申请日：2006-06-30
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C07C221/00 , C07C225/00 , C08C19/22
CPC分类号： B60C1/0016 , C07F1/005 , C07F1/02 , C08C19/44 , C08F36/04 , C08F4/488
摘要： This invention discloses a process for making dilithium initiators in high purity. This process can be conducted in the absence of amines which is desirable since amines can act as modifiers for anionic polymerizations. The dilithium compounds made are highly desirable because they are soluble in aromatic solvents. The present invention also discloses a tire which is comprised of a generally toroidal-shaped carcass with an outer circumferential tread, two spaced beads, at least one ply extending from bead to bead and sidewalls extending radially from and connecting said tread to said beads, wherein said tread is adapted to be ground-contacting, and wherein said tread is a cured the rubber formulation which is comprised of (a) at least one rubbery polymer containing functional groups of the structural formula: wherein R, R′ and R″ can be the same or different, wherein R is selected from the group consisting of hydrogen atoms, alkyl groups, aryl groups, alkaryl groups, and amino aryl groups, and wherein R′ and R″ represent alkyl groups alkyl groups that contain from 1 to 8 carbon atoms, and (b) at least one member selected from the group consisting of carbon black and silica.
摘要翻译：本发明公开了一种制备高纯度二锂引发剂的方法。该方法可以在不存在胺的情况下进行，因为胺可以用作阴离子聚合的改性剂。所制备的二锂化合物是非常需要的，因为它们可溶于芳族溶剂。本发明还公开了一种轮胎，其包括具有外圆周胎面的大致环形胎体，两个间隔开的胎圈，从胎圈到胎圈延伸的至少一个帘布层和从所述胎面径向延伸并将所述胎面连接到所述胎圈的侧壁，其中所述胎面适于与地面接触，并且其中所述胎面是固化的橡胶配方，其由（a）至少一种含有以下结构式的官能团的橡胶状聚合物组成：其中R，R'和R“可以是相同或不同，其中R选自氢原子，烷基，芳基，烷芳基和氨基芳基，其中R'和R“表示含有1至8个碳的烷基基团原子，和（b）选自碳黑和二氧化硅中的至少一种。

84. 发明申请

US20080161489A1 RUBBERY BLOCK POLYMERS CONTAINING POLYLACTONE AND RUBBER COMPOUNDS INCLUDING THE SAME 失效
标题翻译：包含聚合物和橡胶化合物的橡胶块聚合物包括它们
公开(公告)号：US20080161489A1
公开(公告)日：2008-07-03
申请号：US11617342
申请日：2006-12-28
申请人： Adel Farhan Halasa , Abderrahim Khadir , Wen-Liang Hsu , John Robert Zuppo , Mark Weydert
发明人： Adel Farhan Halasa , Abderrahim Khadir , Wen-Liang Hsu , John Robert Zuppo , Mark Weydert
IPC分类号： C08K3/36
CPC分类号： C08F297/04 , C08F297/044 , C08K3/36 , C08K5/548 , C08L53/02 , Y10S152/905 , C08L2666/02 , C08L2666/14
摘要： The present invention is directed to rubbery block polymers containing a polylactone, such as polycaprolactone, methods of making the same, and to rubber compounds containing those block polymers. The rubbery block polymer is an anionically polymerized block polymer defined by A-B, wherein A includes at least one type of polymerized conjugated diene monomer, a polymerized vinyl aromatic monomer, or a mixture thereof and wherein B is a polylactone, such as polycaprolactone, which is hydroxy terminated. The rubbery block polymer may be compounded so to provide, for example, a tire tread with desirable properties for use in an automobile tire. Such rubber compound, for example, can include the rubbery block polymer, an organosilane coupling agent, such as a bis(trialkoxysilyl) alkane, bis(trialkoxysilylalkyl) polysulfide, or mixtures thereof, and silica filler in specified amounts.
摘要翻译：本发明涉及含有聚内酯如聚己酸内酯的橡胶嵌段聚合物，其制备方法以及含有这些嵌段聚合物的橡胶化合物。橡胶嵌段聚合物是由AB定义的阴离子聚合的嵌段聚合物，其中A包括至少一种聚合的共轭二烯单体，聚合的乙烯基芳族单体或其混合物，其中B是聚内酯，例如聚己内酯，羟基封端。可以将橡胶状嵌段聚合物复合以提供例如具有用于汽车轮胎的期望性能的轮胎胎面。例如，这种橡胶化合物可以包括橡胶嵌段聚合物，有机硅烷偶联剂，例如双（三烷氧基甲硅烷基）烷烃，双（三烷氧基甲硅烷基烷基）多硫化物或其混合物，以及指定量的二氧化硅填料。

85. 发明授权

US07064171B1 Non-random styrene-butadiene rubber 失效
标题翻译：无规丁苯橡胶
公开(公告)号：US07064171B1
公开(公告)日：2006-06-20
申请号：US11232685
申请日：2005-09-22
申请人： Adel Farhan Halasa , Wen-Liang Hsu , David Michael Smith, Sr. , Warren James Busch , John Joseph Andre Verthe , Scott Edwards Johnson
发明人： Adel Farhan Halasa , Wen-Liang Hsu , David Michael Smith, Sr. , Warren James Busch , John Joseph Andre Verthe , Scott Edwards Johnson
IPC分类号： C08F236/10
CPC分类号： C08L9/06 , B60C1/0016 , C08F236/10 , C08L7/00 , C08L9/00 , C08L97/005 , Y10S152/905 , C08L2666/02 , C08L2666/08
摘要： The present invention reveals a tire having a tread that is comprised of (1) 30 phr to 80 phr of a non-random styrene-butadiene rubber comprised of polymer chains that are derived from styrene and 1,3-butadiene, wherein from about 10 weight percent to about 50 weight percent of the repeat units in the styrene-butadiene rubber are derived from styrene, wherein from about 60 weight percent to about 90 weight percent of the repeat units in the styrene-butadiene rubber are derived from 1,3-butadiene, wherein from about 30 weight percent to about 50 weight percent of the styrene repeat units are in sequences containing 5 to 20 styrene repeat units, wherein the bound styrene content found in the first half of the polymer chains differs from the bound styrene content found in the second half of the polymer chains by at least 5 weight percent, wherein the styrene-butadiene rubber has a 1,2-vinyl content which is within the range of about 8 percent to about 20 percent, wherein the styrene-butadiene rubber has a number average molecular weight which is within the range of 200,000 to 475,000, and wherein the styrene-butadiene rubber has a glass transition temperature which is within the range of −82° C. to −50° C. and (2) 20 phr to 70 phr of polybutadiene. The tire tread formulation can optionally contain silica and lignin.
摘要翻译：本发明揭示了具有胎面的轮胎，该胎面由（1）30phr至80phr由衍生自苯乙烯和1,3-丁二烯的聚合物链组成的非无规丁苯橡胶组成，其中约10 苯乙烯 - 丁二烯橡胶中重复单元的重量百分比至约50重量％衍生自苯乙烯，其中苯乙烯 - 丁二烯橡胶中重复单元的约60重量％至约90重量％丁二烯，其中约30重量％至约50重量％的苯乙烯重复单元是含有5至20个苯乙烯重复单元的序列，其中在聚合物链的前半部分中发现的结合苯乙烯含量与发现的结合的苯乙烯含量不同在所述聚合物链的后半部分中至少5重量％，其中所述苯乙烯 - 丁二烯橡胶具有在约8％至约20％范围内的1,2-乙烯基含量，其中所述苯乙烯 - 丁二烯 iene橡胶的数均分子量在200,000至475,000的范围内，其中丁苯橡胶的玻璃化转变温度在-82℃至-50℃的范围内，（2 ）20phr至70phr的聚丁二烯。轮胎胎面配方可任选地含有二氧化硅和木质素。

86. 发明授权

US06956093B1 Preparation of syndiotactic polybutadiene, rubber composition and tire with rubber component 有权
标题翻译：间同立构聚丁二烯，橡胶组合物和橡胶组分轮胎的制备
公开(公告)号：US06956093B1
公开(公告)日：2005-10-18
申请号：US10977750
申请日：2004-10-29
申请人： Wen-Liang Hsu , Adel Farhan Halasa
发明人： Wen-Liang Hsu , Adel Farhan Halasa
IPC分类号： C08C2/04 , C08F6/06 , C08F36/06 , C08F136/06 , C08F297/04 , C08L9/00 , C08L9/06 , C08L21/00 , C08L53/02
CPC分类号： C08F36/06 , C08C2/04 , C08F136/06 , C08F297/04 , C08L9/00 , C08L9/06 , C08L21/00 , C08L53/02 , C08F2/42 , C08F4/7096 , C08L2666/08 , C08L2666/04 , C08L2666/02
摘要： The present invention relates to the preparation of syndiotactic 1,2-polybutadiene polymer using a catalyst containing a carbon disulfide in which the polymerizate thereof is treated with hydrogen peroxide, to preparation of a composite of conjugated diene-based elastomer and syndiotactic 1,2-polybutadiene polymer using a catalyst containing a carbon disulfide which the polymerizate thereof is treated with hydrogen peroxide, a rubber composition containing said syndiotactic 1,2-polybutadiene polymer and/or said composite and a tire having at least one rubber component thereof.
摘要翻译：本发明涉及使用含有二硫化碳的催化剂制备间规1,2-聚丁二烯聚合物，其中聚合物用过氧化氢处理，制备共轭二烯系弹性体与间同立构1,2-二烯系弹性体的复合体，使用含有二氯化碳的催化剂的聚丁二烯聚合物，其中聚合物用过氧化氢处理，含有间同立构1,2-聚丁二烯聚合物和/或所述复合材料的橡胶组合物和具有至少一种橡胶组分的轮胎。

87. 发明授权

US06933358B2 Functionalized monomers for synthesis of rubbery polymers 失效
公开(公告)号：US06933358B2
公开(公告)日：2005-08-23
申请号：US10389131
申请日：2003-03-14
申请人： Adel Farhan Halasa , Wen-Liang Hsu , Jin-Ping Zhou , Chad Aaron Jasiunas , Corey Stanton Yon
发明人： Adel Farhan Halasa , Wen-Liang Hsu , Jin-Ping Zhou , Chad Aaron Jasiunas , Corey Stanton Yon
IPC分类号： C07D211/08 , C07D265/30 , C08C19/44 , C08F4/46 , C08F26/06 , C08F126/06 , C08F236/10 , C08F236/14
CPC分类号： C08F236/14 , C08C19/44 , C08F236/10
摘要： This invention discloses a process for synthesizing an amine functionalized monomer that comprises (1) reacting a secondary amine with a 2,3-dihalopropene to produce a vinyl halide containing secondary amine having a structural formula selected from the group consisting of wherein R and R′ can be the same or different and represent allyl, alkoxyl or alkyl groups containing from 1 to about 10 carbon atoms, and wherein X represents a halogen atom, and wherein m represents an integer from 4 to about 10, and wherein X represents a halogen atom; and (2) reacting the vinyl halide containing secondary amine with a vinyl magnesium halide to produce the monomer having a structural formula wherein R and R′ can be the same or different and represent alkyl, allyl or alkoxyl groups containing from 1 to about 10 carbon atoms, and wherein m represents an integer from about 4 to about 10.

88. 发明授权

US06867265B2 Process for improved coupling of rubbery polymers 失效
标题翻译：改进橡胶状聚合物偶联的方法
公开(公告)号：US06867265B2
公开(公告)日：2005-03-15
申请号：US10307187
申请日：2002-11-29
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F4/48 , C08F297/04 , C08F8/00
CPC分类号： C08F297/04 , C08F297/044
摘要： Rubbery polymers made by anionic polymerization can be coupled with tin halides or silicon halides to improve the characteristics of the rubber for use in some applications, such as tire treads. In cases where the rubbery polymer was synthesized utilizing a polar modifier it is difficult to attain a high level of coupling. This invention is based upon the unexpected finding that coupling efficiency can be significantly improved by conducting the coupling reaction in the presence of a lithium salt of a saturated aliphatic alcohol, such as lithium t-amylate. This invention discloses a process for coupling a living rubbery polymer that comprises reacting the living rubbery polymer with coupling agent selected from the group consisting of tin halides and silicon halides in the presence of a lithium salt of a saturated aliphatic alcohol. The lithium salt of the saturated aliphatic alcohol can be added immediately prior to the coupling reaction or it can be present throughout the polymerization and coupling process. Lithium t-amylate reacts with water to form t-amyl alcohol during steam stripping. Since t-amyl alcohol forms an azeotrope with hexane, it co-distills with hexane and can contaminate recycle feed streams. This problem of recycle stream contamination can be solved by using metal salts of cyclic alcohols that do not co-distill with hexane or form compounds during steam stripping which co-distill with hexane. Thus, the use of metal salts of cyclic alcohols is preferred for this reason and because they are considered to be environmentally safe.
摘要翻译：通过阴离子聚合制备的橡胶聚合物可与锡卤化物或卤化硅偶联，以改善用于某些应用中的橡胶的特性，例如轮胎胎面。在使用极性改性剂合成橡胶状聚合物的情况下，难以获得高水平的偶联。本发明基于意想不到的发现，通过在饱和脂肪醇的锂盐如叔戊醇锂的存在下进行偶联反应可以显着改善偶联效率。本发明公开了一种使活性橡胶状聚合物偶合的方法，其包括在饱和脂肪醇的锂盐存在下使活性橡胶状聚合物与选自锡卤化物和卤化硅的偶联剂反应。饱和脂肪醇的锂盐可以在偶联反应之前立即加入，或者可以在整个聚合和偶联过程中存在。在蒸汽汽提期间，叔戊醇钠与水反应形成叔戊醇。由于叔戊醇与己烷形成共沸物，因此与己烷共蒸馏，可能污染再循环进料流。循环流污染的这个问题可以通过使用在与汽油共蒸馏的汽提过程中不与己烷共蒸馏或形成化合物的环醇的金属盐来解决。因此，由于这个原因，优选使用环状醇的金属盐，并且因为它们被认为是环境安全的。

89. 发明授权

US06727311B2 Light weight rubber composition containing clay 失效
标题翻译：轻质橡胶组合物含有粘土
公开(公告)号：US06727311B2
公开(公告)日：2004-04-27
申请号：US10002870
申请日：2001-11-15
申请人： Manoj Ajbani , Wen-Liang Hsu , Adel Farhan Halasa , Ginger Lee , Eric Sean Castner
发明人： Manoj Ajbani , Wen-Liang Hsu , Adel Farhan Halasa , Ginger Lee , Eric Sean Castner
IPC分类号： C08K334
CPC分类号： C08K3/346 , C08K9/04 , Y10S152/905 , C08L19/006
摘要： This invention discloses a rubber composition that is comprised of: (1) an amino group containing rubbery polymer, wherein said amino group containing rubbery polymer contains from about 0.1 weight percent to about 20 weight percent of monomer units containing an amino group, and (2) from about 0.1 phr to about 25 phr of a 2:1 layered silicate clay, wherein the 2:1 layered silicate clay is an organophilic 2:1 layered silicate clay.
摘要翻译：本发明公开了一种橡胶组合物，其包含：（1）含氨基的橡胶状聚合物，其中所述含氨基的橡胶状聚合物含有约0.1重量％至约20重量％的含有氨基的单体单元，和（2 ）约0.1phr至约25phr的2:1层状硅酸盐粘土，其中2:1层状硅酸盐粘土是亲有机质的2:1层状硅酸盐粘土。

90. 发明授权

US06693160B1 Functionalized monomers for synthesis of rubbery polymers 失效
公开(公告)号：US06693160B1
公开(公告)日：2004-02-17
申请号：US10384020
申请日：2003-03-07
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F23814
CPC分类号： C08F236/14 , C08F236/10
摘要： This invention discloses a process for synthesizing an amine functionalized monomer that comprises (1) reacting a secondary amine with a 2,3-dihalopropene to produce a vinyl halide containing secondary amine having a structural formula selected from the group consisting of wherein R and R′ can be the same or different and represent allyl, alkoxyl or alkyl groups containing from 1 to about 10 carbon atoms, and wherein X represents a halogen atom, and wherein m represents an integer from 4 to about 10, and wherein X represents a halogen atom; and (2) reacting the vinyl halide containing secondary amine with a vinyl magnesium halide to produce the monomer having a structural formula wherein R and R′ can be the same or different and represent alkyl, allyl or alkoxyl groups containing from 1 to about 10 carbon atoms, and wherein m represents an integer from about 4 to about 10.

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